CN107946548B - Preparation method of lithium-iron oxide and carbon composite lithium ion battery anode material - Google Patents
Preparation method of lithium-iron oxide and carbon composite lithium ion battery anode material Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention discloses a preparation method of a lithium ion battery anode material compounded by lithium iron oxide and carbon, which relates to the field of battery material preparation, in particular to the field of anode materials of lithium ion batteries, and is characterized in that: fe (Fe) 3 O 4 And (C) preparing Fe with 20% -50% of carbon element content by adopting a mixed iron source, a carbon source, a template agent and a mixed solvent through multiple high-temperature heat treatments 3 O 4 Negative electrode material of/C lithium ion battery, fe coated on surface C 3 O 4 The nano particles are embedded in a carbon conductive network in an elliptic shape or a water drop shape; the mixed iron source is a mixed salt formed by combining ferric salt with mixed salt of ferric chloride, ferric nitrate nonahydrate and ferric sulfate, and the mixed iron source has the advantages of stable structural performance, good safety performance, high specific capacity, excellent rate performance, low price and cycle stability.
Description
Technical Field
The invention relates to the field of battery material preparation, in particular to the field of negative electrode materials of lithium ion batteries.
Background
The lithium ion battery has the advantages of high working voltage, large specific energy, long cycle life, wide working temperature range, no pollution, no memory effect and the like, and is widely applied to the fields of portable electronic equipment, electric tools, space technology, national defense, military and the like. The lithium ion battery cathode material is used as a key component, and has the advantages of high specific capacity, small lithium loss, good reaction reversibility, high battery energy density and good cycle performance. How to increase the capacity of the material and improve the stability and the multiplying power performance of the material is a problem of important research on the cathode material. The negative electrode materials of the lithium ion batteries in the market at present are mainly various graphite carbon materials, such as natural graphite, modified graphite, graphitized mesophase carbon microbeads, soft carbon (such as coke), hard carbon and the like. Energy storage and power batteries require lithium ion batteries with large capacity and high power. The volume specific capacity of graphite is not high enough, lithium is easy to be separated out on the surface of graphite and lithium dendrite is generated during quick charge, potential safety hazard is brought, and the requirement of a power battery is difficult to meet.
Transition metal oxide M x O y The transition metal oxide (m=fe, co, ni, mn, etc.) has theoretically a higher capacity due toThe density of the material is much higher than that of carbon, so that the volume specific capacity of the material is 5-7 times of the theoretical capacity of the carbon material widely applied at present, and the material can bear charge and discharge with higher power, and can meet the requirements of tool batteries and power batteries. These metal oxides react reversibly with lithium metal during charge and discharge: m is M x O y +2yLi + +2ye - ↔xM+yLi 2 O, the metal oxide is reduced into nano simple substance metal in the charging process, and Li is present at the same time 2 O generation of such Li 2 O is electrochemically active and will be re-reduced to elemental lithium in a subsequent discharge. The nanoparticle metal particles generated by the first charge have high electrochemical activity, so the reaction can occur reversibly.
In a series of studies on ion battery anode materials, ferroferric oxide (Fe 3 O 4 ) As a lithium ion battery cathode material, the material has the characteristics of high theoretical capacity, low cost, environmental friendliness and the like, and is concerned by researchers. However, fe 3 O 4 The conductivity deviation of the material is large in volume change in the charge and discharge process, so that the cycle performance and the multiplying power performance of the material are poor, and the practical use of the material is limited.
Disclosure of Invention
The preparation method of the lithium ion battery anode material compounded by the lithium iron oxide and the carbon has the advantages of stable structural performance, good safety performance, high specific capacity, excellent rate performance, low price and cycle stability.
A lithium ion battery cathode material for storing lithium iron oxide and carbon composite is prepared from the following materials in proportion,
7-8 parts of Fe 3 O 4 C, 1-2 parts of carbon black and 1-1.5 parts of binder PVDF
Said Fe 3 O 4 And (C) preparing Fe with 20% -50% of carbon element content by adopting a mixed iron source, a carbon source, a template agent and a mixed solvent through multiple high-temperature heat treatments 3 O 4 Negative electrode material of/C lithium ion battery, fe coated on surface C 3 O 4 The nano particles are embedded in oval shape or water drop shapeIn a carbon conductive network;
the mixed iron source is a mixed salt formed by combining 20-30% of ferric chloride, 10-30% of ferric nitrate nonahydrate and 40-70% of mixed salt of ferric sulfate;
the molar ratio of the carbon source to the mixed iron source is 5:1-10:1, and one or a mixture of more than one of glucose, sucrose, chitosan and citric acid is adopted;
the template agent is one or a mixture of more of sodium chloride, sodium nitrate and sodium sulfate;
the mixed solvent adopts the following components in percentage by mass: 3 to 4 parts of hydrochloric acid with the concentration of 10 percent, 20 to 42 parts of silver carbonate with the concentration of 0.02 to 0.06mol/L, 8 to 12 parts of hydrofluoric acid with the concentration of 5mol/L and 20 to 38 parts of ammonia water with the concentration of 25 percent.
The invention synthesizes Fe coated with surface C by adopting a solution method 3 O 4 Composite material with nanoparticles embedded in an oval or water-drop-shaped carbon conductive network that can avoid Fe 3 O 4 The direct contact of the nano particles and the electrolyte is beneficial to maintaining the material structure and interface stability; at the same time, is coated with Fe 3 O 4 The flexible carbon layer on the surface of the nano-particles can buffer Fe in the charge and discharge process 3 O 4 Mechanical stress due to volume change of/C, suppressing Fe 3 O 4 The pulverization and failure of the nano particles enhance the conductivity of the material and improve the cycle performance of the material to a certain extent. The battery material has high specific capacity, good cycle performance and good multiplying power performance, and is an ideal cathode material for the lithium ion battery with high energy density. The method has the advantages of convenient process operation, no special requirement on experimental environment, no pollution and suitability for expanding reproduction.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1
Step (1) taking mixed salt formed by mixing 25% of ferric chloride, 20% of ferric nitrate nonahydrate and 55% of mixed salt of ferric sulfate;
taking the mol ratio of glucose to the mixed iron source of 6:1
Taking sodium chloride with the mass 7.5 times of that of glucose;
mixing 3.5 parts of 10% hydrochloric acid, 31 parts of 0.02-0.06 mol/L silver carbonate, 10 parts of 5mol/L hydrofluoric acid and 29 parts of 25% ammonia water to obtain a mixed solvent, wherein the mass of the mixed solvent is 5 times that of glucose,
uniformly dissolving a mixed iron source, a carbon source and a template agent in a mixed solvent to obtain a mixture A;
step (2) uniformly stirring the mixture A obtained in the step (1) for 1h at room temperature to obtain a uniform mixed solution B,
step (3), the mixed solution B obtained in the step (2) is placed in a common drying oven at 80 ℃ for drying for 24 hours, and the dried product is ground in an agate mortar, so that a uniform mixture C is obtained;
step (4), placing the dried product of the mixture C obtained in the step (3) into a tube furnace, and performing heat treatment for 2 hours at 800 ℃ under argon atmosphere, wherein the heating rate is 3 ℃/min, so as to obtain a product D;
step (5), placing the product D obtained in the step (4) in a muffle furnace, and performing heat treatment for 6 hours at the temperature of 250 ℃ and under the air atmosphere, wherein the heating rate is 3 ℃/min, so as to obtain a product E;
and (6) washing the product E obtained in the step (5) with deionized water for 3 times, centrifuging and drying.
Example two
Step (1) taking mixed salt formed by mixing 20% of ferric chloride, 10% of ferric nitrate nonahydrate and 70% of mixed salt of ferric sulfate;
taking the mol ratio of glucose to the mixed iron source of 8:1
Taking sodium chloride with the mass 7.5 times of that of glucose;
mixing 3 parts of hydrochloric acid with the concentration of 10%, 20 parts of silver carbonate with the concentration of 0.02-0.06 mol/L, 8 parts of hydrofluoric acid with the concentration of 5mol/L and 38 parts of ammonia water with the concentration of 25% into a mixed solvent, wherein the mass of the mixed solvent is 5 times that of glucose,
uniformly dissolving a mixed iron source, a carbon source and a template agent in a mixed solvent to obtain a mixture A;
step (2) uniformly stirring the mixture A obtained in the step (1) for 1h at room temperature to obtain a uniform mixed solution B,
step (3), the mixed solution B obtained in the step (2) is placed in a common drying oven at 80 ℃ for drying for 24 hours, and the dried product is ground in an agate mortar, so that a uniform mixture C is obtained;
step (4), placing the dried product of the mixture C obtained in the step (3) into a tube furnace, and performing heat treatment for 2 hours at 750 ℃ under argon atmosphere, wherein the heating rate is 5 ℃/min, so as to obtain a product D;
step (5), placing the product D obtained in the step (4) in a muffle furnace, and performing heat treatment for 6 hours at the temperature of 250 ℃ and under the air atmosphere, wherein the heating rate is 5 ℃/min, so as to obtain a product E;
and (6) washing the product E obtained in the step (5) with deionized water for 3 times, centrifuging and drying.
Example III
Step (1) taking mixed salt formed by mixing 30% of ferric chloride, 30% of ferric nitrate nonahydrate and 40% of mixed salt of ferric sulfate;
taking the mol ratio of glucose to the mixed iron source of 8:1
Taking sodium chloride with the mass 7.5 times of that of glucose;
mixing 4 parts of 10% hydrochloric acid, 42 parts of 0.02-0.06 mol/L silver carbonate, 12 parts of 5mol/L hydrofluoric acid and 20 parts of 25% ammonia water to obtain a mixed solvent, wherein the mass of the mixed solvent is 5 times that of glucose,
uniformly dissolving a mixed iron source, a carbon source and a template agent in a mixed solvent to obtain a mixture A;
step (2) uniformly stirring the mixture A obtained in the step (1) for 0.8h at room temperature to obtain a uniform mixed solution B,
step (3), placing the mixed solution B obtained in the step (2) in a common drying oven at 100 ℃ for drying for 24 hours, and grinding a dried product in an agate mortar to obtain a uniform mixture C;
step (4), placing the dried product of the mixture C obtained in the step (3) into a tube furnace, and performing heat treatment for 4 hours at 700 ℃ under argon atmosphere, wherein the heating rate is 2.5 ℃/min, so as to obtain a product D;
step (5), placing the product D obtained in the step (4) in a muffle furnace, and performing heat treatment for 7 hours at 280 ℃ under the air atmosphere, wherein the heating rate is 4 ℃/min, so as to obtain a product E;
and (6) washing the product E obtained in the step (5) with deionized water for 3 times, centrifuging and drying.
Comparative example
Comparative example
Is obtained by the Co.Ltd 3 O 4 ) As a negative electrode material for lithium ion batteries.
Fe prepared in examples one to three, respectively 3 O 4 Uniformly mixing a binder PVDF (10-20) according to the mass ratio of (70-80), wherein the binder PVDF is uniformly mixed, an organic solvent N-methylpyrrolidone (NMP) is used as a dispersing agent, stirring is carried out for 6h to obtain negative electrode slurry, an EC/DEC (volume ratio of 1:1) mixed solution of 1 mol/L LiPF6 is used as electrolyte, a polypropylene porous membrane is used as a diaphragm, and the obtained lithium ion battery silicon-carbon negative electrode materials are assembled into button batteries A1, A2 and A3;
comparative example a button cell B1 was assembled by a conventional method, and a charge and discharge test was performed on a charge and discharge meter.
Table 1 comparison of buckling test results for examples and comparative examples
| Battery cell | A1 | A2 | A3 | B1 |
| Negative electrode material | Example 1 | Example 2 | Example 3 | Comparative example |
| First discharge capacity (mAh/g) | 482.4 | 486.1 | 488.7 | 391.9 |
| First time efficiency (%) | 93.1 | 92.8 | 92.3 | 88.7 |
The foregoing examples illustrate only a few embodiments of the invention and are described in detail herein without thereby limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (1)
1. A preparation method of a lithium ion battery anode material compounded by lithium iron oxide and carbon is characterized by comprising the following steps of: the lithium ion battery cathode material is prepared from the following materials in proportion,
7-8 parts of Fe 3 O 4 C, 1-2 parts of carbon black and 1-1.5 parts of binder PVDF
Said Fe 3 O 4 Preparing carbon element by adopting mixed iron source, carbon source, template agent and mixed solvent through multiple high-temperature heat treatment
Fe with 20-50% element content 3 O 4 Negative electrode material of/C lithium ion battery, surface C coatedFe 3 O 4 The nano particles are embedded in a carbon conductive network in an elliptic shape or a water drop shape;
the mixed iron source is a mixed salt formed by combining 20-30% of ferric chloride, 10-30% of ferric nitrate nonahydrate and 40-70% of mixed salt of ferric sulfate;
the molar ratio of the carbon source to the mixed iron source is 5:1-10:1, and one or a mixture of more than one of glucose, sucrose, chitosan and citric acid is adopted;
the template agent is one or a mixture of more of sodium chloride, sodium nitrate and sodium sulfate;
the mixed solvent adopts the following components in percentage by mass: 3 to 4 parts of hydrochloric acid with the concentration of 10 percent, 20 to 42 parts of silver carbonate with the concentration of 0.02 to 0.06mol/L, 8 to 12 parts of hydrofluoric acid with the concentration of 5mol/L and 20 to 38 parts of ammonia water with the concentration of 25 percent;
the preparation method comprises the following steps:
uniformly dissolving a mixed iron source, a carbon source and a template agent in a proper amount of mixed solvent to obtain a mixture A, wherein the molar ratio of the iron source to the carbon source is 1:5-1:10;
uniformly stirring the mixture A obtained in the step (1) for 0.5-1h at room temperature to obtain a uniform mixed solution B, drying the mixed solution B obtained in the step (2) in a common drying oven at 80-110 ℃ for 24h, and grinding a dried product in an agate mortar to obtain a uniform mixture C;
step (4), placing the dried product of the mixture C obtained in the step (3) into a tube furnace, and performing heat treatment for 2-4 hours at 700-800 ℃ under argon atmosphere, wherein the heating rate is 1-5 ℃/min, so as to obtain a product D;
step (5), placing the product D obtained in the step (4) in a muffle furnace, and performing heat treatment for 4-8 hours at the temperature of 250-350 ℃ under the air atmosphere, wherein the heating rate is 1-5 ℃/min, so as to obtain a product E;
step (6), washing the product E obtained in the step (5) with deionized water for 3 times, centrifugally separating and drying to obtain a target product Fe 3 O 4 /C。
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| CN109786709B (en) * | 2019-01-23 | 2021-01-29 | 东北大学秦皇岛分校 | Ferroferric oxide/carbon composite negative electrode material and preparation method and application thereof |
| CN111554963B (en) * | 2019-02-12 | 2021-04-27 | 成都佰思格科技有限公司 | Lithium ion battery and preparation method thereof |
| CN109841795A (en) * | 2019-03-14 | 2019-06-04 | 电子科技大学 | A kind of preparation method of negative electrode of lithium ion battery |
| CN114772704B (en) * | 2022-04-12 | 2024-03-08 | 哈尔滨工业大学 | Nano iron oxide modified carbon-based electrode and macroscopic-size large-scale preparation method and application thereof |
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| CN102790217A (en) * | 2012-07-26 | 2012-11-21 | 天津大学 | Carbon cladded ferriferrous oxide negative electrode material of lithium ion battery and preparation method thereof |
| CN103219510A (en) * | 2013-03-21 | 2013-07-24 | 华中科技大学 | Lithium battery negative electrode material preparation method and its product |
| CN103435105A (en) * | 2013-08-07 | 2013-12-11 | 浙江凯恩电池有限公司 | Iron oxide/carbon composite lithium ion battery anode material as well as preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102790217A (en) * | 2012-07-26 | 2012-11-21 | 天津大学 | Carbon cladded ferriferrous oxide negative electrode material of lithium ion battery and preparation method thereof |
| CN103219510A (en) * | 2013-03-21 | 2013-07-24 | 华中科技大学 | Lithium battery negative electrode material preparation method and its product |
| CN103435105A (en) * | 2013-08-07 | 2013-12-11 | 浙江凯恩电池有限公司 | Iron oxide/carbon composite lithium ion battery anode material as well as preparation method and application thereof |
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